反应详情

A mixture of methyl 8-(2-bromo-4-fluorobenzenesulfonylamino]-pyrazolo[5,1-a]isoquinoline-7-carboxylate (Intermediate 2, 0.103 g), tris-(dibenzylideneacetone)-dipalladium (0) (0.025 g), tri-tert-butylphosphonium tetrafluoroborate (0.0127 g) and N,N-diethyl-N—((Z)-1-tributylstannanylprop-1-en-3-yl)-amine (Intermediate 3, 0.265 g) in dioxane (3 mL) was irradiated in the microwave at 80° C. for 2 hours. After cooling, the mixture was diluted with ethyl acetate and filtered through Celite. The filtrate was concentrated in vacuo and the residue was purified by chromatography on silica, eluting with a mixture of methanol and DCM with a gradient of 0-20% to give methyl 8-[2-((Z)-3-diethylaminoprop-1-enyl)-4-fluorobenzenesulfonylamino]-pyrazolo[5,1-a]isoquinoline-7-carboxylate (0.030 g).

1. customwas irradiated in the microwave at 80° C. for 2 hours
2. temperatureAfter cooling
3. filtrationfiltered through Celite
4. concentrationThe filtrate was concentrated in vacuo
5. customthe residue was purified by chromatography on silica
6. washeluting with a mixture of methanol and DCM with a gradient of 0-20%